Method for producing a compound containing titanium carbid.



{UNITED sTA'rEs PATENT OFFICE.

AUGUSTE J. 30851 AND WILLIAM I.

MEREDITH, or NIAGARA FALLS, NEW Your,

ASSIGNORS TO THE TITANIUM ALLOY MANUFACTURING COMPANY, NEW YORK,

N. Y.,.A CORPORATION OF No Drawing.

To all whom it may concern Beit known that we, Aucusrn J. Rossr andWILLIAM F. MEREDI H, both citizens of the United States, residing atNiagara Falls, in thev county of Niagara and State of New York, havejointly inventedla Method for Producing a Compound Containing TitaniumCarbid, of which the following is a specification, also originallydisclosed by us in Letters Patent No. 1,039,672, grantedto us September24:, 1912.

Our present inventions relate to the production of essentially metallicsubstances or compounds particularly useful-in the purification orcleansing of metals from therein occluded undesired elements and theircompounds including slags, or in imparting other superior qualities tometals.

The objects of our inventions comprise production of more eflicient suchcompounds, and by methods more rapid, certain and economical thanheretofore, and we attain these objects by our novel method ofproduction as hereinafter disclosed and claimed.

The nature, novelty and scope of our present inventions will be thevbetter understood by reference to the prior art relating to compoundsuseful for the improving or purifying purposes referred to. It isbelieved that these are best exemplified in their highest development,and as now applied on extensive industrial scales, by numerous LettersPatent of the United States heretofore issued to Auguste J. Rossi,ofwhich, for example, No. 609,466, datedAugust23, 1898, discloses theproduction, for the said purposes, of an alloy of iron and titaniumcontaining also some carbon. Inspection of the said Rossi patents and ofthe prior art will, it is believed, disclose that hitherto it has beensupposed that the aforesaid improvements of other metals by aid oftitanium as the effective agent .00 d be successfully ac-'. complishedonly by a metals, .While molten, of an alloy or com pound containingtitanium in its elemental or metallic state. The present industrialpractice of such improvements on extended scales has apparentlyproceeded exclusively on this theory, the methodspractised of producingsuch alloys or compounds, for -instance .those of iron and titanium, aseviqdenced by the Letters Patent referred to, in-

volving procedures carefully guarded to se- Specification of LettersPatent.

dition to such other METHOD r012. rnonuome A ooMP'ouNn CONTAININGTITANIUM onnnrn.

Patented Apr. 21, 1914.

Application filed January 11, 1913. Serial No. 741,372.

conglomerated in very minute sub-divisions with other metal, is, if thecompound so constltuted be added to molten metal to purify or improveit, ultimately as efiicacious, or -more so, than metallic titanium addedas such, and this at considerably less cost to the manufacturer. Thisnovel compound, so containing the car-bid of titanium, as substitute formetallic titanium, possesses, We have found, characteristics renderingit superior, for industrial uses and purposes, to

said alloys of elemental titanium with other metals, as for instance theferro-titanium product of the aforesaid Letters Patent, suchsuperiorities comprising its-comparativelyv economical production, asper the method hereinafter described, and also its comparativestability, or capacity to delay momentarily 'liberation'of the metallictita-- nium, thus enabling less of latter to produce more completepurification owing to its more complete permeation and distributionthroughout the bath during disintegration of the carbid therein beforeactual purification by liberated metallic titanium begins.

It will be understood that, prior to our present invention, thepractised methods of producing alloys of titanium by carbon reduction,as for example per the process described in said Letters Patent No.609,466,

involved application. of temperature, 2'. e. energy, to the chargesufliciently great to insure presence, in the final product, of the mostpossible of metallic titanium; also the addition of substantially nomore carbon than calculated to be suificient to reduce the oxids of saidcharge, and leave in the final product not-to exceed a comparatively"small percentage of uncombined-carbon, 2'. e..carbon in graphitic state,thereby insuring the acquisitlon and reten ion in-the alloy of the Lproducing said. alloys,

greatest amount of metallic titanium derivable from the charge. To thisend, in

the additions of caron were regulated accordingly, and, the temperatureof the bath raised and maintained, at corresponding expense of energy,to insure not only the reduction of the oxids but also the prevention ofcarbids in the final product. This procedure resulted in twoconsiderable items of expense, which our method saves to themanufacturer, viz; the expense of maintaining the temperaturesufiicie'ntly high and long to attain the desired metallic titaniumresult, and also the expensive drafts meanwhile made upon theconstituents of the carbon electrodes employed and also upon thegraphitic walls of the furnace, and aggravated by the aforesaid stintingof the carbon additions to the charge to insure the previously desiredconstitution of the final alloy product. Our novel product, orcomposition, only more effective and economical thanthe said alloys oftitanium for' purifying, or

i observedthat other improvement of metals, but is also easier andcheaper to produce, and therefore correspondingly more desirable anduseful, particularly 1n view of the present magni tude'of operations inmetals being practised by aid of metallic titanium.

We are satisfied that additions of carbid of titanium in isolated formto baths of such metals must prove ineffective to improve them, owingnot'only to the magnitude of the sub-divisions of such carbid, howeverfinelypulverized by any economically practicable mechanical means, butalso to the comparative indissolubility, in the bath, of carbid thusadded by itself alone. We have found, however, that the carbid, if addedin association with other metal, and

in the condition of' much smaller sub-division and homogeneousconglomeration with such metal resulting from our method of production,not only dissolves freely, rapidly, and' homogeneously, throughoutthebath of metal treated, thus permeating it thoroughly, bined carbonsoon thereafter, owing to the existing temperature and other conditions,se a'rates from its content of titanium, thus re easing within the metaltreated, and when and where most needed, a multitude of comparativelyminute particles of free metallic titanium, which then combine with theundesired ele- H ments and compounds present to form new compoundswhich,-as is nowwell understood, accomplishes the desired purification,the surplus of titanium, if any desired, im-

parting to the final productother improved characteristics .for specialuses. It will be.

the addition of the titanic agent in theform of its carbid thus serves,

in a measure, as it were, to postpone the acis thus not 'sirablydiminishing. the

but also that its content of comhomogeneously distributed very theapplication of tion\of the titanium as a purifier until betteropportunity accorded for; its extended and intimate co-mixture withthe-ingredients of the bath, as compared to the hitherto additions ofthe titanium in metallic state when it immediately commences itsreactions 'at the points where introduced and without similaropportunity accorded for prelimi* nary, more uniform, distribution. Itmay be that this increases momentarily the time of treatment required,71. e. the interval in the operation after addition of the purifyingagent, but this, requiring only a fewv minutes, we regard as more thancounterbalanced by the greater opportunity for more evenly distributedaction and purification accorded by the carbid character'in which thetitanium is introduced as above explained, the result including a savingin the total amount of metallic titanium otherwise required to producethe desired final result.

Our said novel purifying compound, possessing the requiredcharacteristics above referred to, may be produced as follows: In afurnace capable of developing and maintaining the required.temperatures, as for example preferably an electric furnace of ordinarytype and construction, such' for in stance as shown and described in U.S. Let- 95 ters Patent to Auguste J. Rossi, No. 802,941, dated October24, 1905, or No. 822,305, dated June 5, 1906, is charged, in suchproportions as may be desired, metal, for example iron,

also' titanium oxid and also carbon, the lat- 10ov ter preferably insuch proportions as not only to satisfy the affinity therefor of theoxygen of said oxid, but also enough to fully satisfy the aflinitytherefor of the therefrom liberated titanium, andalso enough carbon 1besides to insure to the resulting product such uncombined carboncontent as may be desired, these more liberal additions of carbon thanheretofore, resulting also in deformer "expensive losses of carbon-fromthe electrodes and the I graphite of fthe'hearth or crucible.

It will be understood" that instead of the metal, or iron, mentioned,-oxids thereof might be charged, care being, infthatcase, 5 taken toincrease the 'proportion of carbon so asto insureitheir reductionalso.'- The temperature of the charge is then raised, asfby'turning onthe current,1but no higher 1 than .suflicientto oxid, of titanium. Itwill be understood that such rising tem erature wlllresult first in theformationo Javbath of molten metal other than titanium, and

this whether introduced in elemental. or in 5 "oxid form, providedin thelatter case suffiinsure reduction of the no reached, thetemperature mustbe lowered \the graphitic state,

as rapidly as is industrially possible, lest continuation, or even slowdiminution, thereof result in robbing the carbid of its combined carbon,as by latters passing into or making new combinations as with oxidsspeedy lowering of the temperature may be accomplished by tapping thecharge as soon as it has reached the stage mentioned,

and promptly casting the molten product sufliciently distributed ingraphite, or other heat conductive receptacles. After it has thus, orotherwise, been rapidly cooled, our carbid-containing final product isready for use as a purifying, or otherwise improving, addition to bathsof molten metals, to which it may be added in manner substantially asindicated by prevailing practice when ferrotitanium, for example, isused as a purifier.

It will be'understood that our compounds of titanium carbid with othermetals than iron are producible by the method above specificallydescribed, the procedurein each case being substantially the same exceptthat such other desired metal, or its oxid, is substituted for the iron.Thus compounds of carbid of titanium with copper, tin, lead,

zinc, manganese, antimony, etc. may be pro duced for use in thepurification of such metals. Our said compounds. so obtained will befound to comprise the metal of the charge, having therewith intimatelymixed and homogeneously conglomerated minute particles or sub-divisionsof carbid of titanium, its said minute sub-division and association withmetal being as aforesaid, we believe, particularly important, if notindispensable, to the successful action thereafter of the titaniumconstituent of the carbid as a purifying or otherwise improving agent.

It seems unnecessary to further describe the details of operationrequired to produce our said compound, since the necessarilyever-varying character of subordinate details will be readily understoodby those skilled in the metallurgical art. For instance, the proportionsand temperatures of each chargewill, of course, be varied to suitpresent. This required requirements of each particular case and of ofsaid carbid may be'profitably employed,

as 80 per cent. It will be understood that a low content of the carbidmay prove undesirable owing and also as high to the proportionallygreater bulk of the compound. required for purifying. 'On the other handit seems inadvisable to exceed 80% of carbid m the compound because ofinversely prof portional influence of the therewith associatedconstituent metal of the compound when the latter is added as a purifierto a bath of molten metal.

Having now described our invention, what we claim as new anddesire tosecure by Letters Patent is 1. The method of producing a compoundconsisting essentially of metal having therewith intimately mixed andhomogeneously conglomerated minute particles of carbid of titanium whichcomprises first producing a bath of said metal in molten state mixedwith titanium oxid'and carbon, raising the temperature of said bathsuificiently to pro duce therein more of saidcarbid than of metallictitanium, and 'cooling the product so rapidly as to promote retention ofsaid carbid.

2. The method of with intimately mixed and homogeneously conglomeratedminute particles of carbid oftitanium which comprises first producing abath of molten'iron mixed with titanium oxid and carbon, of said bathsulficiently to produce therein more of said carbid than of metallictitanium, and cooling the product so rapidly as to promote retention ofsaid carbid,

AUGUSTE J. ROSSI. WILLIAM F. MEREDITH.

Witnesses WALTER. D. EDMoNDs,

PHILIP C. PECK.

raising the temperatureproducing a compound consisting essentially ofiron having there-

